関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Chloro-2-fluoro-5-(pentyloxycarbonylmethyloxy)nitrobenzene | HCID 14617849 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 4-Chloro-2-fluoro-5-(pentyloxycarbonylmethyloxy)aniline | HCID 14617850 | 75.2% |
反応手順
A mixture of iron powder (115 g), acetic acid (29 g) and water (551 g) was heated at 80° C., and a solution of the compound (III) (132 g) in acetic acid (200 g) was dropwise added thereto in 1 hour, followed by heating under reflux for 5 hours. The reaction mixture was filtered to remove insoluble materials, and the filtrate was extracted with ethyl acetate. The extract was concentrated under reduced pressure. The residue was distilled off under reduced pressure to give 4-chloro-2-fluoro-5-(pentyloxycarbonylmethyloxy)aniline (Compound (II)) (90 g). Yield, 75 b.p., 145°-149° C./0.4 mmHg. m.p., 32°-3420 C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04987247 |
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| 出典データセット | uspto-grants-1991_01 |
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| ORD ID | ord-fa61744c7add4522ab5fde25b4ef6dac |
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| 出典メモ | uspto-grants-1991_01 |
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